CN107892272A - AlH3/ functionalization graphene composite and its preparation method and application - Google Patents
AlH3/ functionalization graphene composite and its preparation method and application Download PDFInfo
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- CN107892272A CN107892272A CN201711005098.XA CN201711005098A CN107892272A CN 107892272 A CN107892272 A CN 107892272A CN 201711005098 A CN201711005098 A CN 201711005098A CN 107892272 A CN107892272 A CN 107892272A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
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- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
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Abstract
A kind of AlH3/ functionalization graphene composite and its preparation method and application, with AlH3It is initiation material with functionalization graphene, AlH is prepared for by solventnonsolvent method at normal temperatures3/ functionalization graphene composite.Including:S1:By AlH3It is configured to suspension A;S2:Configuration feature graphite alkene dispersion liquid B;S3:After A and B are sufficiently mixed, surfactant C, non-polar solven D is added dropwise, completes AlH3With functionalization graphene self assembly.Present invention process is simple, easily operated, is easy to industrialized production, can make AlH using the functionalization graphene of denier3Coat completely and graphene coated amount can adjust, due to graphene excellent mechanical property and chemical stability, do not influenceing AlH3On the premise of hydrogen content, AlH is effectively raised3Security in should having in fields such as propellants.
Description
Technical field
The invention belongs to energetic material field, it can be applicable to propellant, explosive wastewater more particularly, to one kind or other contain
The AlH of energy Material Field3/ functionalization graphene composite, and its improve AlH under normal temperature condition using functionalization graphene3
In the method for energetic material field applicability.
Background technology
Three aluminum hydrides(AlH3)Have that the combustion heat is higher, can produce the advantages of micro-molecular gas relative to aluminium powder, be solid
The ideal fuels of aluminium powder are substituted in composite propellant.According to the calculated results, AlH is used3Instead of aluminium powder, can at least improve solid
The specific impulse 100N.s.kg of body propellant-1, and its combustion chamber and ejection gas temperature are below propellant containing aluminium powder.Therefore,
AlH3High energy additive as solid propellant turns into domestic and international researcher's focus of attention.
In the early 1960s, US military is to AlH3Application militarily is assessed, and finds AlH3Stability
Difference, hydrogen is released during storage, not only reduce the energy of energetic material, and influence the preparation technology and security of energetic material
Energy.Therefore, AlH3Since successfully preparing, always along with to its study on the modification.At present, to AlH3The method master of surface treatment
There are surface passivation method, organic matter and inorganic matter cladding process, ion infiltration method and crystal transfer method etc..Although these methods can
Increase AlH to a certain extent3Stability and security, but normally result in hydrogen content decline, Surface coating it is not fine and close
The problems such as, it is impossible to meet the requirement to its security performance in propellant development process.
Functionalization graphene is oxygen-containing using the carboxyl, hydroxyl and the epoxy radicals isoreactivity that contain in graphene edge and surface
Functional group, chemically reacted by hydroxylating, esterification, carboxylated, sulfonates, amination and fluorination etc. to obtain.Function graphite
Alkene not only has excellent electric property, hot property and the mechanical property that graphene is possessed(Such as high-specific surface area, high intensity, good
Good tribological property etc.), and functionalization graphene also has some unique performances, such as compatibility with organic solvent, dives
It is a kind of preferable surface modifying material in characteristics such as chemical modification, bridging properties.
The content of the invention
To achieve the above object, the invention provides one kind to have hydrogen content height, body after being mixed with propellant usual component
It is the low AlH of sensitivity3/ functionalization graphene composite.
The present invention also aims to provide above-mentioned AlH3The normal temperature preparation method of/functionalization graphene composite,
The present invention prepares AlH using solvent-nonsolvent method3/ functionalization graphene compound, utilize the property that functionalization graphene is excellent
Can, including mechanical performance, heat endurance and higher specific surface area, solve AlH3Security in energetic material application is asked
Topic, or solve other surfaces method of modifying amount of modifier higher, the problem of causing hydrogen content relatively low.
The present invention also aims to provide above-mentioned AlH3/ functionalization graphene composite is in propellant, explosive wastewater
Deng the application in energetic material field.
The invention provides a kind of AlH3/ functionalization graphene composite normal temperature preparation method, comprises the following steps:,
It is characterized in that comprise the following steps:
S1)Under normal temperature condition(20℃), by AlH3Suspension A is configured to, specifically, by AlH3Powder, which is placed in, fills AlH3(Quality
g):Solvent(Volume ml)Than for 1:40~1:In 60 polar solvent and the beaker persistently stirred, AlH is kept3In polar solvent
Suspend, obtain suspension A;
S2)Under normal temperature condition, configuration feature graphite alkene dispersion liquid B, specifically, weigh functionalization graphene, with power 600w,
Time 2h, ultrasonic disperse obtain dispersion liquid B in polar solvent, and the functionalization graphene dosage is step S1)Middle AlH3Quality
0.1wt% ~ 1wt%, the concentration of the functionalization graphene is 1mg/L ~ 100mg/L;
S3)Dispersion liquid B is added dropwise in suspension A, is sufficiently mixed 30min, surfactant C is added dropwise, continues after being added dropwise to complete
After stirring 30min, non-polar solven D is added dropwise, after being added dropwise to complete, filters, clean, be dried to obtain AlH3/ functionalization graphene is multiple
Condensation material;
The step S3)Middle surfactant C is AlH30.02wt% ~ 0.2wt% of mass content;
The step S3)In in non-polar solven D used and step S1 and S2 the volume ratio of polar solvent sum be 1:1 to 10:
1。
Step S1 of the present invention)In polar solvent used be methanol, ethanol, acetonitrile, ethylene glycol, glycerine, in acetone
One or more.
Step S1 of the present invention)Middle mixing speed is 200r/min-1000r/min.
Step S2 of the present invention)In functionalization graphene used be graphene oxide, fluorinated graphene, amino graphite
One kind in alkene or sulfonates graphene;Preferably, AlH shared by functionalization graphene3The ratio of quality be 0.2wt% ~
0.8wt%.
Step S2 of the present invention)In polar solvent used be methanol, ethanol, acetonitrile, ethylene glycol, glycerine, one in acetone
Kind is a variety of.
Step S3 of the present invention)In surfactant C used be polyethylene glycol, polyethylene glycol amine, polyetheramine, one in tween
Kind.
Preferably, surfactant C is AlH30.05wt% ~ 0.1wt% of mass content.
Step S3 of the present invention)Middle surfactant C rate of addition is 1 drop/min ~ 20 drops/min.It is described nonpolar molten
Agent D rate of addition is 60 drops/min ~ 600 drops/min.
Step S3 of the present invention)In non-polar solven D used be petroleum ether, hexamethylene, hexane, heptane, carbon tetrachloride,
One or more in chloroform.
AlH3The sensitivity characteristic of/functionalization graphene is evaluated using collision sensitivity instrument and friction sensitivity instrument, is tested
AlH3/ functionalization graphene and propellant key component GAP/NG/BTTN mass ratioes 1:The sensitivity of 1 mixture.
The present invention, at normal temperatures by solvent-anti-solvent method, realizes AlH using the excellent characteristic of function graphite3With
The controllable self assembly of functionalization graphene, is prepared AlH3/ functionalization graphene composite, AlH of the invention3/ function fossil
Functionalization graphene is evenly coated at AlH in black alkene composite3Surface.Tested by impact sensitivity and friction sensitivity, checking
Its security applied in composite solidpropellant.The AlH of the present invention3/ functionalization graphene composite hydrogen content is high,
System sensitivity is low after being mixed with propellant usual component.
Advantage is the present invention compared with prior art:(1)Functionalization graphene is bigger than surface and AlH3Carry out self assembly,
Dosage is few, and treatment effect is obvious, is easy to industrialized production.(2)Functionalization graphene surface active groups enrich and AlH3With reference to
Power is strong, the difficult separation under strong mechanism.(3)Functionalization graphene is remarkably improved AlH3In solid propellant, explosive wastewater etc.
Applicability in energetic material field.
Embodiment
Following examples be in order to be better described the present invention implementation result, but the present invention be not limited only to following groups implementation
Example.
Embodiment 1
Step 1:Weigh 1gAlH3It is placed in 500ml beaker, accurately measures 50ml ethylene glycol, it is ultrasonic under 200w ultrasonic powers
After 5min, temperature control is solution A with stand-by under 200r/min magnetic agitations at 20 DEG C.
Step 2:2mg graphene oxides are weighed, add 50ml ethylene glycol, the ultrasonic 2h under 600w ultrasonic powers, make oxidation stone
Black alkene is fully dispersed, is B solution.B solution is added drop-wise in solution A, is sufficiently mixed 30min, is AB solution.
Step 3:Take 0.5mg polyetheramine to be added dropwise to 1 drop/min in AB solution, persistently stir 30min, take 200ml rings
Hexane is added dropwise in above-mentioned solution with 60 drops/min, after being added dropwise to complete, obtains black AlH3/ graphene oxide suspension.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 0.2wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:7.0J, friction sensitivity 68%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 2
Step 1:Weigh 2gAlH3It is placed in 1000ml beaker, accurately measures 100ml ethanol, it is ultrasonic under 200w ultrasonic powers
After 5min, temperature control is at 20 DEG C, with stand-by under 300r/min magnetic agitations, is designated as solution A;
Step 2:20mg oxidation graphite alkene is weighed, adds 100ml ethanol, ultrasonic 2h, makes graphite oxide under 600w ultrasonic powers
Alkene is fully dispersed, is designated as B solution.B solution is added drop-wise in solution A, is sufficiently mixed 30min, is designated as AB solution.
Step 3:2mg PEG-400 is taken to be added dropwise to 10 drops/min in AB solution, after being added dropwise to complete, lasting stirring
30min, take 400ml carbon tetrachloride to be added dropwise to 300 drops/min in above-mentioned solution, obtain grey black AlH3/ graphene oxide hangs
Supernatant liquid.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 1wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:8.0J, friction sensitivity 68%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 3
Step 1:Weigh 2gAlH3It is placed in 1500ml beaker, accurately measures 100ml volume ratios as 1:1 is acetonitrile and ethylene glycol
Mixed solvent, under 200w ultrasonic powers after ultrasonic 5min, temperature control is at 20 DEG C, to be treated under 400r/min magnetic agitations
With being designated as solution A;
Step 2:16mg oxidation graphite alkene is weighed, it is 1 to add 100ml volume ratios:1 is the mixed solvent of acetonitrile and ethylene glycol,
Ultrasonic 2h under 600w ultrasonic powers, makes graphene oxide fully dispersed, is designated as B solution.B solution is added drop-wise to 20 drops/min molten
In liquid A, 30min is sufficiently mixed, is designated as AB solution.
Step 3:Take 2mg tween to be added dropwise to 20 drops/min in AB solution, after being added dropwise to complete, persistently stir 30min, take
800ml chloroforms are added dropwise in above-mentioned solution with 200 drops/min, obtain black gray expandable AlH3/ graphene oxide suspension.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 0.8wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:7.8J, friction sensitivity 72%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 4
Step 1:Weigh 2gAlH3It is placed in 1500ml beaker, accurately measures 100ml glycerine, surpasses under 200w ultrasonic powers
After sound 5min, temperature control is at 20 DEG C, with stand-by under 600r/min magnetic agitations, is designated as solution A;
Step 2:10mg oxidation graphite alkene is weighed, adds 200ml glycerine, the ultrasonic 2h under 600w ultrasonic powers, makes oxidation stone
Black alkene is fully dispersed, is designated as B solution.B solution is added drop-wise in solution A, is sufficiently mixed 30min, is designated as AB solution.
Step 3:Take 1mg polyethylene glycol amine to be added dropwise to 5 drops/min in AB solution, after being added dropwise to complete, persistently stir 30min,
It is 1 to take 600ml volume ratios:1 hexane and the mixed solvent of heptane, are added dropwise in above-mentioned solution with 600 drops/min, obtain grey black
Color AlH3/ graphene oxide suspension.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 0.5wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:7.0J, friction sensitivity 76%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For for 2.0J, friction sensitivity 100%.
Embodiment 5
Step 1:Weigh 2gAlH3It is placed in 1500ml beaker, accurately measures 100ml glycerine, surpasses under 200w ultrasonic powers
After sound 5min, temperature control is at 20 DEG C, with stand-by under 500r/min magnetic agitations, is designated as solution A;
Step 2:8mg oxidation graphite alkene is weighed, adds 100ml ethylene glycol, ultrasonic 2h, makes graphite oxide under 600w ultrasonic powers
Alkene is fully dispersed, is designated as B solution.B solution is added drop-wise in solution A, is sufficiently mixed 30min, is designated as AB solution.
Step 3:Take 1mg polyetheramine to be added dropwise to 6 drops/min in AB solution, after being added dropwise to complete, persistently stir 30min,
600ml hexanes are taken, are added dropwise to 600 drops/min in above-mentioned solution, obtain grey black AlH3/ graphene oxide suspension.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 0.4wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:7.0J, friction sensitivity 76%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 6
Step 1:Weigh 2gAlH3It is placed in 1000ml beaker, accurately measures 100ml glycerine, surpasses under 60w ultrasonic powers
After sound 5min, temperature control is at 20 DEG C, with stand-by under 1000r/min magnetic agitations, is designated as solution A;
Step 2:12mg oxidation graphite alkene is weighed, it is 1 to add 100ml volume ratios:1 methanol and glycerine mixed solvent,
Ultrasonic 2h under 600w ultrasonic powers, makes graphene oxide fully dispersed, is designated as B solution.B solution is added drop-wise in solution A, fully
30min is mixed, is designated as AB solution.
Step 3:Take 1mg polyetheramine to be added dropwise to 12 drops/min in AB solution, after being added dropwise to complete, persistently stir 30min,
It is 1 to take 400ml volume ratios:1 hexane and heptane, is added dropwise in above-mentioned solution with 300 drops/min, obtains black gray expandable AlH3/ oxygen
Graphite alkene suspension.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ graphene oxide composite wood
Material, graphene oxide content is 0.6wt%.
Step 5:By AlH3/ graphene oxide compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ graphene oxide/
The impact sensitivity of GAP/NG/BTTN systems is:7.2J, friction sensitivity 74%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 7
Step 1:Weigh 2gAlH3It is placed in 1000ml beaker, accurately measures 100ml glycerine, surpasses under 200w ultrasonic powers
After sound 5min, temperature control is at 20 DEG C, with stand-by under 500r/min magnetic agitations, is designated as solution A;
Step 2:8mg fluorinated graphenes are weighed, add 100ml glycerine, ultrasonic 2h, makes graphene oxide under 600w ultrasonic powers
It is fully dispersed, it is designated as B solution.B solution is added drop-wise in solution A, is sufficiently mixed 30min, is designated as AB solution.
Step 3:0.4mg PEG-400 is taken to be added dropwise to 10 drops/min in AB solution, after being added dropwise to complete, lasting stirring
30min, 400ml petroleum ethers are taken, be added dropwise to 600 drops/min in above-mentioned solution, obtain grey AlH3/ fluorinated graphene suspends
Liquid.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after gray precipitate things successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ fluorinated graphene composite wood
Material, fluorinated graphene content is 0.4wt%.
Step 5:By AlH3/ fluorinated graphene compound and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With matter
Measure ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ fluorinated graphene/
The impact sensitivity of GAP/NG/BTTN systems is:7.8J, friction sensitivity 70%, AlH3The impact sensitivity of/GAP/NG/BTTN systems
For 2.0J, friction sensitivity 100%.
Embodiment 8
Step 1:Weigh 2gAlH3It is placed in 1000ml beaker, accurately measures 100ml acetone, it is ultrasonic under 200w ultrasonic powers
After 5min, temperature control is at 20 DEG C, with stand-by under 500r/min magnetic agitations, is designated as solution A;
Step 2:The aminated graphenes of 8mg are weighed, it is 1 to add 100ml volume ratios:1 acetone and acetonitrile mixed solvent, in 600w ultrasounds
Ultrasonic 2h under power, makes graphene oxide fully dispersed, is designated as B solution.By B solution into solution A, 30min is sufficiently mixed, is remembered
For AB solution.
Step 3:0.5mg PEG-400 is taken to be added dropwise to 2 drops/min in AB solution, after being added dropwise to complete, lasting stirring
30min, 400ml heptane is taken, be added dropwise to 200 drops/min in above-mentioned solution, obtain black gray expandable AlH3/ aminated graphene suspends
Liquid.
Step 4:After above-mentioned suspension is carried out into centrifugation 10 minutes, the black gray expandable sediment after centrifugation is taken successively to use second
Alcohol, deionized water cleaning, then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtain dry AlH3/ aminated graphene
Composite, aminated graphene content are 0.4wt%.
Step 5:By AlH3/ aminated graphene complex and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With
Mass ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ amido graphite
The impact sensitivity of alkene/GAP/NG/BTTN systems is:7.5J, friction sensitivity 72%, AlH3The shock of/GAP/NG/BTTN systems
Sensitivity is 2.0J, friction sensitivity 100%.
Embodiment 9
Step 1:Weigh 2gAlH3It is placed in 1000ml beaker, accurately measures 100ml acetone, it is ultrasonic under 200w ultrasonic powers
After 5min, temperature control is at 20 DEG C, with stand-by under 300r/min magnetic agitations, is designated as solution A;
Step 2:The sulfonates graphenes of 8mg are weighed, add 100ml acetone, ultrasonic 2h, makes graphene oxide under 600w ultrasonic powers
It is fully dispersed, it is designated as B solution.By B solution into solution A, 30min is sufficiently mixed, is designated as AB solution.
Step 3:0.8mg PEG-400 is taken to be added dropwise to 5 drops/min in AB solution, after being added dropwise to complete, lasting stirring
30min, take 400ml carbon tetrachloride to be added dropwise to 500 drops/min in above-mentioned solution, obtain black AlH3/ sulfonates graphene hangs
Supernatant liquid.
Step 4:By above-mentioned suspension carry out centrifugation 10 minutes after, take centrifugation after black precipitate successively using ethanol,
Deionized water is cleaned, and then in 30 DEG C of vacuum drying ovens, vacuum heat-preserving 24h, obtains dry AlH3/ sulfonates graphene is compound
Material, sulfonates graphene content are 0.4wt%.
Step 5:By AlH3/ sulfonates graphene complex and poly- nitrine glycerin ether/nitroglycerine(GAP/NG/BTTN)With
Mass ratio 1:1 is well mixed, and impact sensitivity is carried out to mixture and friction sensitivity is tested, is as a result shown:AlH3/ sulfo group graphite
The impact sensitivity of alkene/GAP/NG/BTTN systems is:7.5J, friction sensitivity 72%, AlH3The shock of/GAP/NG/BTTN systems
Sensitivity is 2.0J, friction sensitivity 100%.
Above-described embodiment is that present disclosure is further described, but this should not be interpreted as into the scope of the present invention
It is only limitted to embodiment.It is all that the scope of the present invention is belonged to based on the technology that the above is realized.
Claims (10)
- A kind of 1. AlH3The preparation method of/functionalization graphene composite, it is characterised in that comprise the following steps:S1)Under normal temperature condition, by AlH3Suspension A is configured to, specifically, by AlH3Powder, which is placed in, fills AlH3(Quality g):It is molten Agent(Volume ml)Than for 1:40~1:In 60 polar solvent and the beaker persistently stirred, AlH is kept3Suspended in polar solvent, Obtain suspension A;S2)Under normal temperature condition, configuration feature graphite alkene dispersion liquid B, specifically, weigh functionalization graphene, with power 600w, Time 2h, ultrasonic disperse obtain dispersion liquid B in polar solvent, and the functionalization graphene dosage is step S1)Middle AlH3Quality 0.1wt% ~ 1wt%, the concentration of the functionalization graphene is 1mg/L ~ 100mg/L;S3)Dispersion liquid B is added dropwise in suspension A, is sufficiently mixed 30min, surfactant C is added dropwise, continues after being added dropwise to complete After stirring 30min, non-polar solven D is added dropwise, after being added dropwise to complete, filters, clean, be dried to obtain AlH3/ functionalization graphene is multiple Condensation material;The step S3)Middle surfactant C is AlH30.02wt% ~ 0.2wt% of mass content;The step S3)In in non-polar solven D used and step S1 and S2 the volume ratio of polar solvent sum be 1:1 to 10: 1。
- 2. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S1)In polar solvent used be methanol, ethanol, acetonitrile, ethylene glycol, glycerine, the one or more in acetone.
- 3. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S1)Middle mixing speed is 200r/min-1000r/min.
- 4. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S2)In functionalization graphene used be graphene oxide, fluorinated graphene, amination graphene or sulfonates graphene in It is a kind of;AlH shared by functionalization graphene3The ratio of quality is 0.2wt% ~ 0.8wt%.
- 5. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S2)In polar solvent used be methanol, ethanol, acetonitrile, ethylene glycol, glycerine, the one or more in acetone.
- 6. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S3)In surfactant C used be polyethylene glycol, polyethylene glycol amine, polyetheramine, one kind in tween;Surfactant C is AlH3 0.05wt% ~ 0.1wt% of mass content.
- 7. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S3)Middle surfactant C rate of addition is 1 drop/min ~ 20 drops/min;The non-polar solven D rate of addition is 60 drops/min ~ 600 drops/min.
- 8. AlH according to claim 13The preparation method of/functionalization graphene composite, it is characterised in that:The step Rapid S3)In non-polar solven D used be petroleum ether, hexamethylene, hexane, heptane, carbon tetrachloride, the one or more in chloroform.
- A kind of 9. AlH described in claim 1-83AlH prepared by the preparation method of/functionalization graphene composite3/ function Graphite alkene composite.
- A kind of 10. AlH described in claim 93Application of/functionalization graphene the composite in propellant, explosive wastewater.
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CN109019507A (en) * | 2018-09-03 | 2018-12-18 | 黎明化工研究设计院有限责任公司 | A method of improving three aluminium hydride thermostabilisations |
CN111072708A (en) * | 2019-12-02 | 2020-04-28 | 西安近代化学研究所 | graphene-Schiff base metal complex and preparation method thereof |
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